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SIMPLE DISTILLATION Simple Distillation is the process of boiling a liquid mixture/solution and condensing the vapour to obtain a pure

liquid. [which means, separating liquids from the solution] :) PROCEDURE 1. 2. 3. 4. Solution mixture is heated in a flask until the mixture boils. Pure liquid turns into a vapour and leaves the flask. Vapour is then cooled in a condenser which changes back into liquid. Pure liquid collected is called the distillate and is collected in a conical flask. HOW DOES SIMPLE DISTILLATION WORK?

1. In the distillation flask, liquid boils and enters the condenser. 2. In the condenser, vapour condenses to pure liquid. 3. Pure liquid is collected as distillate. http://separationtechnique-distillation.blogspot.in/ Simple Distillation In simple distillation, a liquid is boiled and the vapors work through the apparatus until they reach the condenser where they are cooled and reliquify. Liquids are separated based upon their differences in boiling point. Two important things to note: 1) the tip of the thermometer must be correctly positioned slightly below the center of the condenser to accurately reflect the temperature of the vapors (see above left) and 2) the water supply should be connected to the lower port in the condenser and the drainage tube connected to the upper (in the picture on the right the right tube is connected to the water supply and the red tube is a drainage tube). Also be sure to use the thin-walled tubing and not the heavy walled vacuum tubing. Be very careful that your water lines do not come in direct contact with your hot plate, as the lines could melt resulting in a flood. Be sure to clamp both the round bottom boiling flask and the collection tube. Knocking over your collection tube at the end of the experiment if VERY frustrating. Below is a diagram of assembly: Generally, boiling stones will be added to the boiling flask to ensure even boiling. It is also wise to use some type of clamps to connect the various pieces of the distillation apparatus together. For low boiling liquids, enough heat may be provided simply by resting your flask on the hot plate (as shown above). You can also insulate your boiling flask and Claisen adaptor with aluminum foil. For higher boiling liquids it may be necessary to use an oil or sand bath to reach higher temperatures. Fractional Distillation The setup for a fractional distillation is very similar to that for simple distillation. The only difference is the addition of a fractional distillation column, usually packed with some material of high surface area that produces a more efficient separation than the simple distillation. The same advice regarding the thermometer placement, clamping, and hook-up of the water tubes in the simple distillation also apply to the fractional distillation. As this apparatus is larger, practice additional caution to be sure that no glassware is broken or product loss. The choice whether to use the simple or the fractional setup will depend on the compounds that you are trying to separate. Obviously, the simple distillation setup is simpler and the distillation generally will be quicker than the fractional. However, the fractional setup is more efficient at separating liquids with fairly similar boiling points and at times is required. http://www.wfu.edu/chem/courses/organic/distill/distillation.htm Fractional Distillation (Adapted from Mohrig, pp. 118-121) Fractional distillation is a technique used when separating a mixture of two liquids that do not "behave" well enough to use simple distillation. In this case simple distillation would not be enough to fully separate the two liquids. The distillate would contain a majority of one liquid but would still contain a little of the second. To further separate this resulting distillate, one would need to redistill this mixture. Depending on the two liquids in question, many simple distillations would be required to obtain pure liquid. Fractional distillation essentially performs these "redistillations" automatically in a portion of the fractional distillation apparatus called the fractionating column. As the mixture boils, it turns to vapor and rises up the column. It reaches a certain point up the column and condenses. It then turns to vapor again and rises a little bit further up the column. This continues until the vapor rises all the way up the column and condenses in the condenser. At this point, the liquid has been completely purified. Procedure The procedure for fractional distillation is very similar to that of simple distillation. Once you have set up your fractional distillation apparatus, place the liquid to be distilled in the distilling flask. The flask should be no more than two-thirds full at the start of the distillation because the contents may foam and boil over. Remember to place one or two boiling stones in the flask to promote even boiling. Ensure that all joints are tight. Turn on the water for the condenser. Only a small stream of water is needed; too much water pressure will cause the tubing to pop off. Turn on the Variac and the distillation can begin. As always, never boil the flask to dryness because, in some cases, high-boiling explosive peroxides can become concentrated. Stop the distillation when a small amount of liquid is left in the distilling flask. Turn off the Variac and remove the heating mantle to allow the flask to cool more quickly.

http://academics.wellesley.edu/Chemistry/chem211lab/Orgo_Lab_Manual/Appendix/Techniques/FractionalDistill/fractional_distill. html How does distillation work? Distillation works by exploiting the different boiling temperatures of liquids. To separate two or more liquids by distillation, you first heat them in a flask. The more volatile liquid (the liquid with the lower boiling point) will typically evaporate first and the vapor will pass into a condensing column, where it can revert into a liquid (condense) on the cool glass where it trickles into a collection flask. Heating further will cause the less volatile liquids to evaporate and distill at higher temperatures. The two main kinds of distillation are simple distillation and fractional distillation, and both are used widely. What is simple distillation? The setup for a simple distillation is shown in Figure 1. A simple distillation apparatus consists of a boiling flask (roundbottom flask) attached to an adapter holding a thermometer (to determine the boiling temperature of the liquid). The adapter connects to a condenser into which cold water is constantly passed through. The condenser leads into a collection flask for the purified liquid. What is fractional distillation? Fractional distillation is essentially the same as simple distillation except that a fractionating column is placed between the boiling flask and the condenser. The fractionating column is usually filled with glass or plastic beads. These beads improve the separation between the liquids being distilled. The reason that fractional distillation gives better separation between the liquids is because the glass beads in the fractionating column provide "theoretical plates" on which the refluxing liquid can condense, re-evaporate, and condense again, essentially distilling the compound over and over. The more volatile liquids will tend to push towards the top of the fractionating column, while lower boiling liquids will stay towards the bottom, giving a better separation between the liquids. Of course, the more theoretical plates that you add to a column (the more surfaces or beads), the longer the distillation will take (typically), and the more energy required to keep reevaporating liquid in the fractionating column (this is more of a concern in industrial distillations than in an academic lab where energy cost is not a major cause for worry). So, simple or fractional? The choice of whether to use fractional distillation or simple distillation depends on the two liquids being separated. Typically, using simple distillation is preferrable because the apparatus is, well, simpler, and a simple distillation typically goes faster than a fractional distillation (and requires less energy). On the other hand, fractional distillation gives better separation between the liquids. The choice of whether to use simple or fractional distillation, then, depends usually on the difference in boiling temperatures between the two liquids. If there is a large difference in the boiling points o (>70 C)between the two liquids then simple distillation is probably the best option. On the other hand, if there is only a small temperature difference between the two liquids a fractional distillation is the preferrable option. Simple distillation simpler setup than fractional faster distillation times consumes less energy than fractional distillation requires the liquids to have large boiling point differences o (>70 C) gives poorer separation than fractional distillation only works well with relatively pure liquids Fractional distillation much better separation between liquids than simple distillation can more readily purify complex mixtures than simple distillation more complicated setup than simple distillation takes longer for liquids to distill consumes more energy than simple distillation

Advantages

Disadvantages

Best used for:

separating relatively pure liquids with separating complex mixtures of liquids large boiling differences or liquids with smaller boiling point separations. with solid impurities

http://www.chemhelper.com/distillation.html What Is the Purpose of the Fractionating Column? Answer The fractionating column is essential for the purpose of fractional distillation of liquids. Usually, the outer jacket is used in order to stop heat loss from happening during the distillation process. It also ensures that the temperature is distributed evenly throughout the length of the column. http://www.ask.com/question/what-is-the-purpose-of-the-fractionating-column